US6544889B2 - Method for tungsten chemical vapor deposition on a semiconductor substrate - Google Patents

Method for tungsten chemical vapor deposition on a semiconductor substrate Download PDF

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US6544889B2
US6544889B2 US09/768,151 US76815101A US6544889B2 US 6544889 B2 US6544889 B2 US 6544889B2 US 76815101 A US76815101 A US 76815101A US 6544889 B2 US6544889 B2 US 6544889B2
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tungsten
deposition
sih
sccm
substrate
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Hans Vercammen
Joris Baele
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AMI Semiconductor Belgium BVBA
Alcatel Lucent SAS
Deutsche Bank AG New York Branch
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/06—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material
    • C23C16/08—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material from metal halides
    • C23C16/14—Deposition of only one other metal element
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
    • H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
    • H01L21/285—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation
    • H01L21/28506—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers
    • H01L21/28512—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic Table
    • H01L21/28556—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic Table by chemical means, e.g. CVD, LPCVD, PECVD, laser CVD
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
    • H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
    • H01L21/285—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation
    • H01L21/28506—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers
    • H01L21/28512—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic Table
    • H01L21/28568—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic Table the conductive layers comprising transition metals

Definitions

  • This invention relates to a method for chemical vapor deposition of a layer of tungsten (W) on a semiconductor substrate.
  • tungsten on a semiconductor substrate such as a silicon oxide wafer which may have portions of an integrated circuit structure already formed therein, such as, for example one or more transistors, is an integral part of most semiconductor fabrication processes.
  • An insulating layer mostly a silicon oxide layer has usually been formed over this substrate and has been previously patterned to provide openings or vias to underlying portions of the integrated circuit structure.
  • Chemical vapor deposited W has been used as a conducting material to fill contact holes or via holes.
  • the tungsten layer covers the complete substrate surface and is then etched or polished away, except from the holes.
  • tungsten layer cannot be deposited by chemical vapor deposition directly on a silicon oxide layer, an intermediate layer with a good adhesion for both the insulating layer and tungsten, for instance a titanium nitride (TiN) layer on top of titanium is deposited.
  • TiN titanium nitride
  • the tungsten is usually deposited through the reduction of tungsten hexafluoride (WF 6 ) in a two-steps process.
  • the steps are different in pressure set points and used reductor, being in the first step mainly silane (SiH 4 ) and then hydrogen (H 2 ) only.
  • the largest part of the film is deposited by H 2 reduction.
  • U.S. Pat. No. 5,028,565 of APPLIED MATERIALS, Inc., Santa Clara, Calif., LISA discloses such method wherein tungsten is deposited on a wafer heated from about 350 to about 525° C. in a vacuum chamber wherein the pressure is maintained from 2.67 to 101.32 kPa (from about 20 to about 760 Torr).
  • a combination is used of WF 6 gas, an inert carrier gas such as Ar, nitrogen and hydrogen.
  • the flow rate of WF 6 is from about 20 to about 200 standard cubic centimeters per minute (hereafter abbreviated as sccm).
  • the flow rate of the inert carrier Ar is from about 100 to about 5000 sccm, and the flow rate of nitrogen is from about 10 to about 300 sccm.
  • the hydrogen flow rate is from about 300 to about 3000 sccm.
  • the N 2 in the gas mixture has been found to increase the reflectivity of the deposited layer which facilitates the use of photolitography in a subsequent patterning step, and to decrease the surface roughness.
  • U.S. Pat. No. 5,028,565 discloses however also that, especially when the intermediate layer is titanium nitride, it is important to form first a nucleation layer with from about 5 to about 50 sccm of WF 6 , from about 5 to about 50 sccm silane (SiH 4 ), from about 500 to about 3000 sccm of Ar and from about 20 to about 300 sccm of N 2 .
  • Literature unanimously confirms the impossibility to obtain a tungsten film with good qualities, especially a good step coverage, a good layer uniformity and a low via resistance, without these two steps.
  • the step coverage is the ratio of the thickness of the tungsten film at the side wall at half depth of the trench or contact hole and the nominal tungsten film thickness or the thickness of top layer.
  • EUI SONG KIM et al. for instance mention in their article “Studies on the nucleation and growth of chemical-vapor-deposited W on TiN substrates”, published in MATERIALS SCIENCE AND ENGINEERING, B 17 (1993) 137-142, that since it is not easy to nucleate W on TiN by H 2 reduction of WF 6 , it is now common to initiate nucleation of W by SiH 4 reduction first and then grow W film to the required thickness by H 2 reduction.
  • the hydrogen reduction gives better step coverage than the silane reduction, but the deposition rate of the hydrogen reduction method is significantly lower. Consequently, the second step in the tungsten deposition is therefore without SiH 4 as in the actual method recommended by the above mentioned company APPLIED MATERIALS, INC.
  • This method comprises a soak step with SiH 4 , to saturate and passivate the underlying layer, a nucleation step at a pressure of 4.00 kPa (30 Torr), wherein 30 sccm WF 6 is reduced by means of a mixture of 1000 sccm H2 and SiH 4 in a flow ratio WF 6 /SiH 4 of 2, and a bulk deposition step at a second pressure of 12.00 kPa (90 Torr) wherein sccm WF 6 is reduced by means of 700 sccm H 2 alone.
  • the wafer is heated to 475° C. during the tungsten deposition. An extra pressurizing step is necessary between both steps as there is a difference in pressure.
  • An object of the invention is to provide a method for tungsten chemical vapor deposition which is more simple and cheaper and has a higher deposition rate than the above mentioned prior art methods while a more simple deposition system may be used, and whereby the characteristics of the tungsten film such as the step coverage, the via resistance, the reflectivity etc. are at least equal to or better than these of a film obtained via the prior art methods.
  • this object is accomplished in a method for tungsten chemical vapor deposition on a semiconductor substrate, comprising positioning said substrate within a deposition chamber, heating said substrate and depositing under low pressure the tungsten on the substrate by contacting the latter with a mixture of gases flowing through the deposition chamber comprising tungsten hexafluoride (WF 6 ), hydrogen (H 2 ) and at least one carrier gas, characterized in that the mixture of gases comprises also silane (SiH 4 ) with such a flow rate that the flow ratio WF 6 /SiH 4 is from 2.5 to 6, the flow rate of WF 6 being from 30 to 60 sccm, while the pressure in the deposition chamber is maintained from 0.13 to 5.33 kPa (I and 40 Torr).
  • WF 6 tungsten hexafluoride
  • H 2 hydrogen
  • carrier gas characterized in that the mixture of gases comprises also silane (SiH 4 ) with such a flow rate that the flow ratio WF 6 /SiH 4 is from 2.5 to 6,
  • the tungsten deposition may be carried out in a single step.
  • Reaction efficiency is high, what results in high deposition rate and low gas consumption. Also the gas cost is low. There are less toxic gases and the overall quality of the tungsten film may be improved with respect to the prior art two step methods.
  • hydrogen is preferably supplied with a flow rate of 500 to 2000 sccm.
  • the temperature to which the substrate is heated depends amongst others on the chamber but is preferably situated between 400 and 495° C., but may be extended to lower temperatures, what however results in a lower deposition rate.
  • Carrier gases may be Ar and N 2 as in the prior art methods.
  • FIG. 1 schematically shows a deposition system for applying the method according to the invention
  • FIG. 2 shows a block diagram illustrating the steps of the method of the invention
  • FIG. 3 shows experimental results of the thickness D and the step coverage SC, when varying the rates of the SiH 4 and WF 6 flows,
  • FIG. 4 shows experimental results of the influence of the WF 6 /SiH 4 ratio on the step coverage of the deposited W layer
  • FIG. 5 shows experimental results, derived from FIG. 3, of the deposition rate, as a function of the WF 6 and SiH 4 flow rates.
  • the deposition according to the invention of a tungsten (W) film on a substrate, more particularly a wafer 1 of semiconductor material, such as silicon, already covered with an insulating silicon oxide layer and an intermediate layer of TiN, is carried out in a commercially available chemical vapor deposition chamber 2 which is mounted in a deposition system.
  • FIG. 1 is a schematic representation of a typical existing one-chamber chemical vapor deposition system which may be used for applying the invention.
  • the deposition chamber 2 has a vacuum port 3 coupled to a vacuum pump 4 through a pressure control device 5 .
  • the system comprises a number of supply lines 6 - 10 coupled to specific sources (not shown) for supplying respectively tungsten hexafluoride (WF 6 ), reducing gas hydrogen (H 2 ), reducing gas silane (SiH 4 ), inert carrier gas argon (Ar), and carrier gas nitrogen (N 2 ).
  • WF 6 tungsten hexafluoride
  • H 2 reducing gas hydrogen
  • SiH 4 reducing gas silane
  • Ar carrier gas nitrogen
  • the flow rate of gas through these supply lines 6 - 10 is controlled by flow controllers 11 .
  • the supply lines 6 and 7 for WF 6 and the carrier gas N 2 are coupled to a manifold 12
  • the supply lines 8 , 9 and 10 for SiH 4 , H 2 and Ar, respectively are coupled to a second manifold 13 .
  • Both manifolds 12 and 13 supply a distribution head 14 inside the chamber 2 through a common gas line 15 .
  • a support 16 having a bottom and upstanding edges is installed inside the deposition chamber 2 .
  • channels 17 may traverse the support 16 , which channels 17 are connected to supply lines 18 for so-called edge gases, more particularly a mixture of controlled flow rates of H 2 and Ar, ensuring the same thickness of the tungsten film at the edges of the wafer 1 as in the center.
  • a heating means 19 for instance a heating resistance, is incorporated in the support 16 for heating the wafer 1 .
  • step 21 the chamber 2 is pumped down through the vacuum port 3 until a predetermined base pressure, which is for instance less than 0.003 kPa (20 milliTorr), and in step 22 , a wafer 1 is placed on the support 16 inside the chamber 2 , while the chamber 2 is further pumped down to said base pressure.
  • a predetermined base pressure which is for instance less than 0.003 kPa (20 milliTorr)
  • step 23 the chamber 2 is pressurized with inert gases Ar and N 2 , provided through the lines 10 and 7 , to a pressure from 0.13 kPa to 5.33 kPa (1 to 40 Torr) determined by the pressure control device 5 .
  • the wafer I As soon as the wafer I is placed on the support 16 , it is heated to a temperature of 400 to 495 20 C. due to its contact with the support 16 which has been heated to said temperature by the heating means 19 .
  • the heating has been indicated in FIG. 2 as step 24 but it is clear that heating starts already and could even be completed during step 23 .
  • the heating means 19 are activated from the start of the method and as long as wafers 1 are subsequently covered by a film of tungsten.
  • a layer of W is deposited by opening the mass flow controllers 11 in the supply lines 6 and 7 so that WF 6 is mixed with a flow of N 2 in the manifold 12 , while the flow controllers 11 in the supply lines 8 , 9 and 10 are opened and SiH 4 and H 2 gases are mixed in the manifold 13 with a flow of Ar.
  • the mass flow controllers 11 determine the flow rate of the different gases.
  • Flow rates of Ar and N 2 are not critical and Ar may for example be dispensed at flow rates from 800 to 3000 sccm and N 2 at flow rates from 10 to 400 sccm. These flow rates may be higher during the pressurization step 23 than during the deposition step.
  • WF 6 is supplied with such flow rate that the ratio WF 6 /SiH 4 is from 2.5 to 6, with a flow rate from 30 to 60 sccm.
  • a flow ratio WF 6 /SiH 4 below 2.5 results in a loss of step coverage, while a flow ratio above 6 results in an increase of stress, a drop in reflectivity, and a lower reaction efficiency. Too much SiH 4 will result in a WF 6 gradient in the hole or trench, decreasing the step coverage.
  • H 2 is supplied with a flow rate from 500 to 2000 sccm. This flow rate is not critical.
  • the support 16 is provided with channels 17 , during step 25 , an edge flow from 0 to 500 sccm H 2 added to a flow of Ar is supplied through these channels 17 .
  • the pressure control device 5 ensures that the above mentioned pressure from 0.13 to 5.33 kPa, is maintained in chamber 2 during the deposition of W. These limits are critical since at a pressure lower than 0.13 kPa, the deposition rate will be too small, while at pressures higher than 5.33 kPa, gas nucleation will take place in the space above the wafer 1 .
  • the chamber 2 is purged in step 26 with Ar and N 2 gases, the flow rates of which may be higher than during the deposition step 25 , after which the chamber 2 is pumped down in step 27 .
  • step 28 the wafer 1 is removed from the chamber 2 .
  • the chamber 2 may again be purged with Ar and N 2 and is then ready to be pumped down for another depositing a W film on another wafer 1 and the above mentioned steps may be repeated.
  • the step coverage is excellent, even for the steepest trenches and the deposition rate is almost doubled with respect of the know methods and being up to 643 nm/min.
  • the complete deposition of W takes places in one step. There is only one pressure during deposition and consequently no pressurizing step between depositions. Only one set of gas settings is required.
  • the flow rates of WF 6 and SiH 4 are critical and adjusted by relatively expensive mass flow controllers 11 which are difficult to calibrate. As the flow rate does not have to be changed during the tungsten deposition, one flow controller for each of these gases is sufficient. In the known two-step methods, two controllers are needed for the WF 6 as there is a low flow and a high flow, which is more expensive.
  • a first step 21 the chamber 2 is pumped down to a pressure of 0.003 kPa (20 milliTorr), and again after a silicon wafer 1 , having a layer of TiN previously formed thereon over an silicon oxide layer, is introduced in the CVD chamber 2 and placed on the support 16 which is maintained at a temperature of 475° C.
  • the chamber 2 is pressurized at a pressure of approximately 4.00 kPa (30 Torr) by means of approximately 2800 sccm Ar and approximately 300 sccm N2.
  • the deposition itself is performed by supplying a flow rate of approximately 1000 sccm H 2 , approximately 50 sccm WE 6 and approximately 15 sccm SiH 4 so that the ratio WF 6 /SiH 4 is approximately 3.3, while maintaining a flow rate of approximately 800 scm Ar and approximately 300 sccm N 2 .
  • a H 2 edge flow of approximately 50 sccm is supplied through channels 17 in order to obtain a more uniform tungsten film.
  • the chamber 2 is purged with 2500 sccm Ar and 300 scam N 2 and pumped down to a pressure of 0,003 kPa, and the wafer 1 is removed.
  • the deposition time was 60.2 s, compared to 78.0 s for a standard method with 30 sccm WF 6 , 15 sccm SiH 4 and 1000 sccm H 2 at a pressure of 4.00 kPa (30 Torr) during nucleation and 95 sccm WF 6 and 700 sccm H 2 and no SiH 4 during bulk deposition.
  • the WF 6 consumption was reduced with 30% with respect to said standard method. Stress and reflectivity were good.
  • a short pre-nucleation step may be added before the depositing step 25 , possibly between the added soak step and the depositing step 25 , by reducing during a few seconds, for example 1 to 7 seconds, the flow rate of WF 6 so that the flow ratio WF 6 /SiH 4 is reduced to about 2, the other parameters remaining the same.
  • This pre-nucleation step is much shorter, for example 1 to 7 seconds compared to the nucleation step in the known methods which take about 20 seconds.
  • results are shown in FIGS. 3 to 5 .
  • layer thickness curves D drawn in thin solid lines
  • step coverage curves SC drawn in thin dashed lines
  • WF 6 /SiH 4 ratio The influence of the WF 6 /SiH 4 ratio on the step coverage is explicitly depicted in FIG. 4 . From the latter figure it is clear that ratios lower than 2 result in a very bad step coverage, lower than 50%. Step coverage becomes excellent from ratios above 3.3.
  • the layer thickness D is used for calculating the deposition rate, as shown in FIG. 5 .
  • Deposition rate is expressed in Angstrom/minute (6.10 ⁇ 9 m/sec). Highest deposition rates are thus obtained with the highest flow rates.
  • the deviation from literature can probably be caused by the mixed kind of chemistry used in these tests: H 2 /SiH 4 /WF 6 , while in most cases only separate chemistries were used.

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US09/768,151 2000-12-28 2001-01-24 Method for tungsten chemical vapor deposition on a semiconductor substrate Expired - Lifetime US6544889B2 (en)

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EP00403705 2000-12-28
EP00403705.7 2000-12-28
EP00403705A EP1219725B1 (de) 2000-12-28 2000-12-28 Verfahren zur chemischen Dampfablagerung von Wolfram auf einem Halbleitersubstrat

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US20080003797A1 (en) * 2006-06-29 2008-01-03 Hynix Semiconductor Inc. Method for forming tungsten layer of semiconductor device and method for forming tungsten wiring layer using the same

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US20130224948A1 (en) * 2012-02-28 2013-08-29 Globalfoundries Inc. Methods for deposition of tungsten in the fabrication of an integrated circuit
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US11810766B2 (en) 2018-07-05 2023-11-07 Applied Materials, Inc. Protection of aluminum process chamber components
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EP1219725B1 (de) 2005-08-17
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US20020086110A1 (en) 2002-07-04
EP1219725A1 (de) 2002-07-03
DE60022067T2 (de) 2006-06-01
CN1366334A (zh) 2002-08-28
ATE302294T1 (de) 2005-09-15

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